CN204170452U - A kind of separation and purification system of organic synthesis feed liquid - Google Patents
A kind of separation and purification system of organic synthesis feed liquid Download PDFInfo
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- CN204170452U CN204170452U CN201420462991.0U CN201420462991U CN204170452U CN 204170452 U CN204170452 U CN 204170452U CN 201420462991 U CN201420462991 U CN 201420462991U CN 204170452 U CN204170452 U CN 204170452U
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Abstract
The utility model relates to a kind of separation and purification system of organic synthesis feed liquid, this separation and purification system comprises the crystal system and solid-liquid separation system that set gradually from front to back, and described crystal system is discharged crystallizer (MSMPR pattern crystallizer) guide shell crystallizer of connecting (DTB crystallizer) by mix suspending-product mix and formed; Described separation and purification system also comprises the liquid processing system processed the waste liquid of solid-liquid separation system extraction, and it comprises the desalter and film condensing device that set gradually from front to back.Separation and purification system synthesis of the present utility model make use of crystallization apparatus, membrane separation device and electrodialysis plant etc. and carries out separation and purification to organic synthesis feed liquid, also can the waste liquid produced be reclaimed fully and be utilized, improve the efficiency of separation and purification and the purity of product and yield, decrease the discharge of waste liquid, manufactureization is strong, cost is low, is particularly suitable for the application in iminodiacetonitrile is produced.
Description
Technical field
The utility model, for the device systems of chemical field, relates to a kind of separation and purification system of organic synthesis feed liquid.
Background technology
Organic synthesis is a kind of major way that chemical industry obtains target product, and its reacted reaction material liquid system forms primarily of target product, residual raw material and accessory substance.Industrially, how separation and purification is carried out with efficient, highly purified acquisition target product to reaction feed liquid, and to greatest extent waste liquid, waste residue is recycled, with industrial efficiency and cost closely bound up.And the lab scale in laboratory is compared with industrialized large-scale production, and it is also more difficult that the state modulator of the latter and the homogeneity of reaction system control.Therefore, how designing one is enclosed within industrialization large-scale production, can carry out the system of efficient separation and purification, farthest improve product yield, purity to organic synthesis feed liquid, and waste liquid and waste residue are recycled fully, there is huge industrialization meaning.
The separation and purification of an organic synthesis feed liquid generally includes the step of crystallization and Separation of Solid and Liquid.The crystallizer adopted is generally the crystallizing tank with temperature control and agitating device, and traditional handicraft gets brilliant mode after usually adopting the heating of primary crystal, mother liquor concentrated again.Because product has higher solubility in water, cause getting brilliant rate lower; Meanwhile, because mother liquor, in heating concentration process, all kinds of chemical reaction occurs, cause its quality to decline fast, thus cannot continue to utilize, raffinate can only as wastewater treatment, and namely mother liquor utilization rate is low, and waste water generation is large.The equipment for separating liquid from solid adopted is generally centrifuge, suction filtration machine, rejection filter machine etc., and operation relates to that filter cake rinses, the problem such as product loss in filtrate.In a word, the yield of the product that the final separation and purification of these equipment obtains and purity, more depend on reaction material liquid system itself, and complicated operation, waste liquid, waste residue are not easy to be recycled.
For the organic synthesis feed liquid of iminodiacetonitrile, its organic synthesis principle is as follows:
Main reaction:
Side reaction:
After above-mentioned reaction terminates, the organic synthesis feed liquid system of acquisition at least comprises residual ammonia and hydroxyacetonitrile, iminodiacetonitrile and accessory substance thereof.To be separated from this reaction feed liquid and obtain iminodiacetonitrile, need ammonia to be converted into inorganic salts and remove, and as much as possible mother liquor is recycled, to improve finished product yield, reduce discharging of waste liquid.China granted patent CN1331844C discloses a kind of preparation technology of iminodiacetonitrile, it finally obtains yield more than 90%, purity is more than 98%, can find out according to embodiment, the lifting of its ultimate yield and purity depends primarily on the control of synthetic reaction condition, last separation and purification operation does not produce contribution function to yield and purity, and reason is just that it uses conventional separation and purification device and method.
The shortcoming existed based on above-mentioned existing technology and needs, the separation and purification system of the utility model to organic synthesis feed liquid is improved.
Utility model content
In view of this, the utility model first provides a kind of separation and purification system that can improve the organic synthesis feed liquid of separation and purification efficiency, product yield and purity.
For achieving the above object, the technical solution of the utility model is:
A separation and purification system for organic synthesis feed liquid, comprises the crystal system and solid-liquid separation system that set gradually from front to back, and described crystal system is the continuous crystallizing system of at least two-stage crystallizer composition, is connected in series between described crystallizer.
Further, described crystal system is discharged crystallizer (MSMPR pattern crystallizer) guide shell crystallizer of connecting (DTB crystallizer or DP crystallizer) by mix suspending-product mix and is formed, or discharge crystallizer by guide shell crystallizer series hybrid suspension-product mix to form, or discharge crystallizer by two or more mix suspending-product mix to be composed in series, or be composed in series by two or more guide shell crystallizer.
MSMPR pattern crystallizer is the abbreviation that mix suspending-product mix discharges (Mixed Suspension-MixedProduct Removal) crystallizer, be characterized in mixing cmpletely within it, any material level in crystallizer is made to be set up the suspension density of crystal and size distribution is all homogeneous, and the suspension density of its magma of product of to discharge from crystallizer and size distribution also identical with in device, namely indiscriminate to varigrained crystal when discharge, and be different from classification discharge.Fig. 1 is shown in by the feature sketch of the utility model MSMPR pattern crystallizer.DTB crystallizer is the abbreviation of guide shell crystallizer (Drabt Tube Babbled), is a kind of typical magma internal-circulation type crystallizer.In crystallization process, the degree of supersaturation of solution, the uniformity consistency of temperature of charge and speed of agitator and film-cooled heat are the deciding factors affecting product grains size and appearance form.DTB crystallizer have employed special paddle, and temperature, rotating speed of agitator are adjustable, easily realize system automatic control system, to adapt to the requirement of various material crystallization, the structure of its uniqueness and operation principle determine it and have the features such as heat transfer efficiency is high, configuration is simple, convenient operation and control, good operational environment.DP crystallizer is the modified of DTB type, and the outer survey of its guide shell is also provided with one group of propeller blade, and crystal particle mean size is increased, and production capacity improves.Carry out Crystallization Separation by the combination of above-mentioned MSMPR pattern crystallizer, DTB crystallizer, DP crystallizer to organic synthesis feed liquid, the product crystal average grain diameter that crystallization obtains can reach more than 0.3mm, and size is even, and uniformity is high; Meanwhile, because crystalline quality is higher, carry out the product after solid-liquid separation through centrifuge, its water content directly can reach quality index, can save product drying step, thus save human and material resources in a large number.
Further, this separation and purification system also comprises the liquid processing system processed the liquid of solid-liquid separation system extraction, and this liquid processing system comprises the desalter and film condensing device that set gradually from front to back; The filtrate (liquid of described solid-liquid separation system is connected with the import of desalter, and the desalinization liquor outlet of described desalter is connected with the import of film condensing device.Wherein, described desalter is used for carrying out desalination to the liquid of solid-liquid separation system extraction, and film condensing device is used for concentrating the liquid after desalter desalination.Described desalter comprises device etc. corresponding to the methods such as counter-infiltration (RO), electrodialysis, diffusion dialysis, forward osmosis, preferred electrodialysis plant or diffusion dialysis device, particularly electrodialysis plant.Described film condensing device comprises device corresponding to the methods such as counter-infiltration, ultrafiltration, nanofiltration.Wherein, described counter-infiltration in principle water be uniquely by the material of film; Particularly all dissolvings and the material of suspension are trapped.This system adopts the technology such as UF membrane, electrodialysis separation, and in mother liquor, product recovery rate promotes, and product yield is significantly improved; Meanwhile, this system produces without the concentrated raffinate of traditional handicraft, and cost for wastewater treatment reduces greatly.
Further, described desalter is electrodialysis plant or diffusion dialysis device.
Further, described solid-liquid separation system comprises the concentrator and centrifuge that set gradually for more than a pair.Described concentrator is the solid-liquid separating equipment based on gravitational settling effect, be generally the cylindrical shape shallow slot being built up the band cone end by concrete, timber or metal welding fishplate bar as structural material, feed liquid carries out sedimentation wherein, and top is more peace and quiet clarified solution (overflow), and bottom is thick feed liquid.Described centrifuge can be in suspended centrifuge, leaf filter and continuous centrifugal machine one or more.Wherein, described continuous centrifugal machine belongs to vertical centrifugal discharging filter screen flow-guiding type centrifuge.During work, material enters in centrifuge by top, tripper is continuously inserted material in flow-guiding channel, under the influence of centrifugal force, material flows downward along flow-guiding channel, in flow process, penetration by liquid filter screen enters liquid-collecting bin, and solid material is then discharged into the solid collection storehouse of bottom along flow-guiding channel.Utilize centrifugal force, continuous centrifugal machine completes centrifugal filtration and centrifugal discharge simultaneously, and the angle of flow-guiding channel can arbitrarily adjust, thus can change the length of passage, control the time of staying of material in flow-guiding channel, the moisture content of solid material is controlled to optimum state.
Further, described solid-liquid separation system comprises the one-level concentrator, suspended centrifuge, secondary concentrator and the leaf filter that set gradually; The described charging aperture of one-level concentrator is connected with the discharging opening of crystal system, the thick material outlet of underflow of one-level concentrator is connected with the charging aperture of suspended centrifuge, and the top stream purified liquor outlet of one-level concentrator is connected with the charging aperture of secondary concentrator with the filtrate (liquid of suspended centrifuge; The thick material outlet of underflow of described secondary concentrator is connected with the charging aperture of crystal system, and the top stream purified liquor outlet of secondary concentrator is connected with the charging aperture of leaf filter; The filtrate (liquid of described leaf filter is connected with the charging aperture of desalter.This form that specifically arranges being " concentrator set gradually for more than a pair and centrifuge ", dense by secondary, fully isolate the crystal in crystalline mixture, thin magma can be back to crystal system crystallization again, isolated filtrate impurity is also less, filtrate enters in follow-up desalination and concentration operation, and also less to the damage of equipment, equipment is more durable.
Further, the concentrated solution outlet of described film condensing device is connected with the charging aperture of centrifuge and/or crystal system crystallizer.That is, reclaim the washing of this concentrate for filter cake, or return of value crystallizer carries out the crystallization of product again.
Further, be provided with decolouring system before described crystal system, the destainer outlet of described decolouring system is connected with the charging aperture of crystal system; Or be provided with decolouring system between described solid-liquid separation system and desalter, now, the filtrate (liquid of described solid-liquid separation system is connected with the import of decolouring system, and the destainer outlet of decolouring system is connected with the import of desalter again.Decolouring system is provided with for carrying out decolouring removing impurities to organic synthesis feed liquid before described crystal system; Decolouring system is provided with for carrying out decolouring removing impurities to the liquid of solid-liquid separation system extraction between described solid-liquid separation system and desalter.
Further, described decolouring system is made up of the ultrafiltration apparatus of connecting and nanofiltration device.Ultrafiltration (UF) is macromolecule component (HMWC), and as protein, suspended solid are trapped, and all lower molecular weight components are freely by the process of film; Nanofiltration (NF) retains the negatively charged ions exceeding monovalence in theory, as sulfate, phosphate (in the present invention, can retain the inorganic salts in feed liquid), and by the anion of unit price.According to bulk of molecule and shape, nanofiltration also can retain neutral, dissolved matter and positive charge ion.Decolouring system adopts the combination of ultrafiltration (UF)+nanofiltration (NF), that is: treat that destainer is first through hyperfiltration treatment, remove the suspension part macromolecule impurity in solution; Ultrafiltration permeate enters nanofiltration separation, successively removes impurity in solution and part inorganic salts through the NF membrane of larger membrane aperture and less membrane aperture; Nanofiltration permeate continues on in production, and trapped fluid is then by being atomized burning disposal after evaporation and concentration.
Further, filter or filtrate collecting tank is also provided with before described desalter, the filtrate (liquid of described solid-liquid separation system is connected with the import of filter or filtrate collecting tank respectively, and the purified liquor outlet of described filter or filtrate collecting tank is connected with the import of desalter again; When being provided with decolouring system after solid-liquid separation system, described filter is the pretreatment part of decolouring system, and the filtrate (liquid of described solid-liquid separation system is connected with the import of filter, and the purified liquor outlet of filter is connected with the import of decolouring system again.Described filter or filtrate collecting tank, for filtering the liquid of solid-liquid separation system extraction or leaving standstill clarification; When being provided with decolouring system after solid-liquid separation system, described filter is the pretreatment part of decolouring system, and the liquid of solid-liquid separation system extraction enters the decolouring of decolouring system again after filtering.For the latter, e.g., filter now consists of: strainer, ultrafilter and nanofiltration device, and the charging aperture of described strainer is connected with the filtrate (liquid of centrifuge, and the filtrate discharging opening of strainer is connected with the charging aperture of ultrafilter; The filtrate (liquid of described ultrafilter is connected with the charging aperture of nanofiltration device; The described filtrate (liquid of nanofiltration device is connected with the charging aperture of desalter.
Further, the precipitation outlet of described filter or filtrate collecting tank is connected with the charging aperture of crystal system.When using strainer, the charging aperture of described strainer flows purified liquor outlet with the top of described concentrator and is connected, and the precipitation discharging opening of described strainer is connected with the charging aperture of crystallizer.The precipitation that aforesaid filtering plant or filtrate collecting tank obtain can import crystallizer, and use as crystal seed, product fully reclaims and also improves total yield of products.
In addition, the utility model also provides the separation and purification system of another organic synthesis feed liquid, there is the feature of the separation and purification system of above-mentioned organic synthesis feed liquid, but wherein said crystal system is replaced by single crystallizer, or the crystal system that described crystal system is composed in parallel by two or more crystallizer is replaced.Particularly, described crystallizer can be MSMPR pattern crystallizer, DTB crystallizer, DP crystallizer etc.
Device systems mentioned in the separation and purification system of above-mentioned organic synthesis feed liquid and device, if those skilled in the art can infer reasonable increase, omission, replacement or rotine positioning adjustment, all should be included in design of the present utility model; Equally, some auxiliary equipment do not mentioned in detail in this system and device, as the setting of the devices such as heating, cooling, pump, basin, every those skilled in the art can expect, also should be included in design of the present utility model.As, the above-mentioned feeder mentioned and strainer, object collects liquid and for standing clarification or filter liquide further, it reasonably omits or by the replacement of other devices, is all included in design of the present utility model.
The separation and purification system of above-mentioned organic synthesis feed liquid can be used for the separation and purification of multiple organic synthesis product feed liquid, and these feed liquids mainly refer to the mixed liquor containing organic products and a large amount of inorganic salts.Preferably, described separation and purification system is used for the separation and purification of iminodiacetonitrile synthesis feed liquid, iminodiacetic acid synthesis feed liquid, glycine synthesis feed liquid or methionine synthesis feed liquid.
Relevant to the separation and purification system of the organic synthesis feed liquid of above-mentioned utility model, the utility model also provides a kind of waste water utilization fully and can improve the recycling system of the waste liquid produced in the organic synthesis feed liquid separation and purification of product yield.
For achieving the above object, the technical solution of the utility model is:
A recycling system for the waste liquid produced in the separation and purification of organic synthesis feed liquid, comprises the filter, desalter and the film condensing device that set gradually from front to back; Described desalter is connected with the liquid outlet of filter, and described film condensing device exports with the desalinization liquor of desalter and is connected; Or comprise the filtrate collecting tank, desalter and the film condensing device that set gradually from front to back; Described desalter is connected with the outlet of feeder, and described film condensing device exports with the desalinization liquor of desalter and is connected.Described feeder plays a part to collect waste liquid, can omit or be replaced by other tank body.
Further, the apparatus system that described separation and purification adopts comprises the decolouring system, crystal system and the solid-liquid separation system that set gradually from front to back; Described solid-liquid separation system is made up of the concentrator set gradually from front to back and centrifuge; Described concentrator is provided with the thick material outlet of underflow and top stream purified liquor outlet, and the thick material outlet of described underflow is connected with centrifuge.
Further, described decolouring system is made up of the ultrafiltration apparatus of connecting and nanofiltration device.
Or, after crystallization is located in above-mentioned decolouring, e.g., before the filtrate desalination of centrifuge, carry out desolventing technology, namely complete this operation by filter.Particularly, described filter is made up of the strainer set gradually from front to back, ultrafilter and nanofiltration device; The filtrate discharging opening of described strainer is connected with the charging aperture of ultrafilter; The filtrate (liquid of described ultrafilter is connected with the charging aperture of nanofiltration device; The described filtrate (liquid of nanofiltration device is connected with the charging aperture of desalter.
Further, the apparatus system that described separation and purification adopts comprises the crystal system and solid-liquid separation system that set gradually from front to back; Described solid-liquid separation system is made up of the concentrator set gradually from front to back and centrifuge; Described concentrator is provided with the thick material outlet of underflow and top stream purified liquor outlet, and the thick material outlet of described underflow is connected with centrifuge; The charging aperture of described strainer is connected with the filtrate (liquid of centrifuge.
Further, the charging aperture of described strainer also flows purified liquor outlet with the top of described concentrator and is connected.
Further, the discharge of filter residues mouth of described strainer is connected with the charging aperture of crystal system.Described filter residue enters crystal system and uses as crystal seed.
Further, the concentrated solution outlet of described film condensing device is connected with the charging aperture of centrifuge and/or crystal system.Described concentrate is used for washing leaching cake, or enters crystal system and extract product further.
Advantageous Effects of the present utility model is:
The utility model has fully utilized CGS Continuous Grain Silicon, electrodialytic technique and membrane separation concentration technology etc. and has carried out separation and purification to organic synthesis feed liquid, and sufficient recovery and utilization have been carried out to the waste liquid produced, improve the efficiency of separation and purification and the purity of product and yield, decrease the discharge of waste liquid, manufactureization is strong, cost is low.Be embodied in following aspect:
(1) by the continuous crystallisation of MSMPR pattern crystallizer, DTB crystallizer or DP crystallizer, product crystal average grain diameter can reach more than 0.3mm, and size is even, and uniformity is high; Meanwhile, because crystalline quality is higher, carry out the product after solid-liquid separation through centrifuge, its water content directly can reach quality index, can save product drying step.With regard to product water content, traditional production technology due to product crystal grain little, Size Distribution is wide, cause product centrifugal filter cake water content on average more than 6.0%, this technique is due to lifting (the average crystal grain diameter increase of product crystalline quality, crystal size distribution scope is narrower), for iminodiacetonitrile, product filter cake can be made to be less than the moisture of 0.5% (w/w%) by means of only centrifugation, greatly be better than the quality index of Grade A moisture≤3.0% (w/w%) in GB/T23958-2009 " industrial iminodiacetonitrile ", thus centrifugal follow-up product drying operation in omission traditional handicraft, enormously simplify production procedure, reduce artificial consumption.
(2) prior art is again got brilliant mode after adopting heating concentrated to product crystalline mother solution and is processed, because product has higher solubility in water, cause getting brilliant rate lower, simultaneously, because mother liquor, in heating concentration process, all kinds of chemical reaction occurs, cause its quality to decline fast, thus cannot continue to utilize, raffinate can only as wastewater treatment.Or prior art is taken out adopting repeatedly the mode of evaporation and concentration, consumes a large amount of steam.On the whole, mother liquor utilization rate is low, and waste water generation is large.The present invention adopts the technology such as electrodialysis, membrane separation concentration to carry out abundant recovery and reuse to crystalline mother solution, product yield, quality all have remarkable lifting, for the production of iminodiacetonitrile, in reactant liquor, product extraction efficiency is promoted to more than 95% by 80%, the main content of product rises to 97% by 95%, production efficiency is high, and production cost is low.
(3) wastewater flow rate obviously declines, and for the production of iminodiacetonitrile, product wastewater flow rate per ton is about 0.15m
3be only 1/10 of former technique, and waste water be high concentration without salting liquid, be easy to burning disposal; Compared with prior art, the inorganic salts entering waste water are separated, achieve recycling, reduce wastewater treatment difficulty simultaneously.
(4) production overall process becomes continuous operation from intermittently operated, and be easy to realize whole-course automation and control, artificial quantity required obviously reduces, and labour intensity greatly reduces, and production cost reduces.
(5) said system and method are applied to the production of iminodiacetonitrile, and product quality is significantly improved, and product extraction efficiency is high, decreases waste discharge, reduces production cost.
Accompanying drawing explanation
Fig. 1 is the structural representation (in figure, a-b is charging aperture, and c-f is discharging opening, and g is cylindrical shell, and h is inner draft tube, and i is agitating device, and j is at the bottom of " W " type or at the bottom of ellipse head) of MSMPR pattern crystallizer;
Fig. 2 is the equipment flowsheet (in figure, before decolouring system is located at crystal system) of the separation and purification system of a kind of organic synthesis feed liquid of the utility model;
Fig. 3 is a kind of structural representation of Fig. 2 equipment;
Fig. 4 is the concrete equipment flowsheet of one of solid-liquid separation system in Fig. 2;
Fig. 5 is a kind of structural representation of Fig. 4 equipment;
Fig. 6 is the equipment flowsheet (in figure, after decolouring system is located at crystal system, namely decolour synchronously complete by during filtration devices) of the separation and purification system of the another kind of organic synthesis feed liquid of the utility model;
Fig. 7 is a kind of structural representation of Fig. 6 equipment;
Fig. 8 is equipment flowsheet when utilizing the utility model systematic position purifying iminodiacetonitrile and flow direction of material figure (eliminating storage tank in figure);
Fig. 9 is a kind of structural representation of Fig. 8 equipment and flow direction of material;
Figure 10 is the concrete equipment flowsheet of one and the flow direction of material figure of solid-liquid separation system in Fig. 8;
Figure 11 is a kind of structural representation of Figure 10 equipment and flow direction of material.
Detailed description of the invention
As shown in Figures 2 and 3, a kind of organic synthesis feed liquid separation and purification system of the present utility model and liquid waste treatment system thereof, comprise the liquid processing system 3 that the decolouring system 4, crystal system 1, solid-liquid separation system 2 and the waste liquid to solid-liquid separation system 2 extraction that set gradually from front to back process.Described decolouring system 4 is made up of the ultrafiltration apparatus of connecting and nanofiltration device.Described crystal system 1 is made up of MSMPR pattern crystallizer series connection DTB crystallizer, and this crystal system also can be single stage crystallizer or traditional crystallization kettle is formed.Described solid-liquid separation system 2 comprises the concentrator and centrifuge that arrange from front to back.Described liquid processing system 3 comprises the filter 301 (this filter 301 also can be cancelled, or is replaced by a feeder 6, plays a part to collect filtrate, clarification), desalter 302 and the film condensing device 303 that set gradually from front to back; Described filter 301 is connected with the filtrate (liquid of centrifuge, and described desalter 302 is connected with the liquid outlet of filter 301, and described film condensing device 303 exports with the desalinization liquor of desalter 302 and is connected.The concentrated solution outlet of described film condensing device 303 is connected with the charging aperture of centrifuge and/or crystallizer.
The organic synthesis feed liquid separation and purification system of Fig. 2 and liquid waste treatment system thereof are operationally, the material flow direction is wherein: first organic synthesis feed liquid enters decolouring system 4 and to decolour removal of impurities, enter MSMPR pattern crystallizer and the crystallization of DTB crystallizer more successively, the material liquid mixture of crystallization enters solid-liquid separation system 2 again and carries out fractional defecation, centrifugation; The filtrate of centrifugal acquisition is filtered by filter 301 successively, desalter 302 desalination, and film condensing device 303 concentrates, and finally obtains concentrate and is back to centrifuge washing leaching cake, or be back to the crystallization again of DTB crystallizer.
Preferred as one of the present utility model, as shown in Figure 4 and Figure 5, solid-liquid separation system 2 wherein comprises the one-level concentrator 201, suspended centrifuge 202, secondary concentrator 203 and the leaf filter 204 that set gradually from front to back.The top flow export of described one-level concentrator 201 is connected with secondary concentrator 203 charging aperture, and underflow outlet is connected with suspended centrifuge 202 charging aperture; Described suspended centrifuge 202 filtrate (liquid is connected with secondary concentrator 203 charging aperture.Secondary concentrator 203 pushes up flow export and is connected with leaf filter 204 charging aperture, and underflow outlet is connected with decolouring system 4 or crystal system 1; The outlet of leaf filter 204 is connected with the charging aperture of desalter 302.
The solid-liquid separation system 2 of Fig. 4 operationally, the material flow direction is wherein: send in one-level concentrator 201 by the magma of DTB crystallizer extraction, promote solid content to target component, underflow is sent into suspended centrifuge 202 and carry out solid-liquid separation, the filter cake obtained is packaged to be finished product by centrifuge automatic discharging, vibrations tape transport and automatic packaging machine.The filtrate that the top stream of one-level concentrator 201 and suspended centrifuge 202 obtain proceeds in secondary concentrator 203, and the underflow of secondary concentrator 203 is back to decolouring system 4 or crystal system 1 extracts product again; The top stream of secondary concentrator 203 is sent into leaf filter 204 and is filtered, and the clear liquid obtained enters desalter 302 desalination.
As shown in Figure 6 and Figure 7, a kind of organic synthesis feed liquid separation and purification system of the present utility model and liquid waste treatment system thereof, comprise the liquid processing system 3 that the crystal system 1, solid-liquid separation system 2 and the waste liquid to solid-liquid separation system 2 extraction that set gradually from front to back process.Described crystal system 1 is made up of MSMPR pattern crystallizer series connection DTB crystallizer.Described solid-liquid separation system 2 comprises the concentrator and centrifuge that arrange from front to back.Described liquid processing system 3 comprises the filter 301, desalter 302 and the film condensing device 303 that set gradually from front to back; Described filter 301 is connected with the filtrate (liquid of centrifuge, and described desalter 302 is connected with the liquid outlet of filter 301, and described film condensing device 303 exports with the desalinization liquor of desalter 302 and is connected.Described filter 301 is made up of the strainer set gradually from front to back, ultrafilter and nanofiltration device; The charging aperture of described strainer is connected with the filtrate (liquid of centrifuge, and the filtrate discharging opening of strainer is connected with the charging aperture of ultrafilter; The filtrate (liquid of described ultrafilter is connected with the charging aperture of nanofiltration device; The filtrate (liquid of described nanofiltration device is connected with the charging aperture of desalter 302.The concentrated solution outlet of described film condensing device 303 is connected with the charging aperture of centrifuge and/or DTB crystallizer.In addition, the charging aperture of described strainer also flows purified liquor outlet with the top of described concentrator and is connected, and the discharge of filter residues mouth of described strainer is connected with the charging aperture of DTB crystallizer.
The organic synthesis feed liquid separation and purification system of Fig. 6 and liquid waste treatment system thereof are operationally, the material flow direction is wherein: organic synthesis feed liquid enters continuous crystallizing system, and the material liquid mixture of crystallization enters solid-liquid separation system 2 again and carries out fractional defecation, centrifugation; The filtrate of centrifugal acquisition is filtered by filter 301 successively, desalter 302 desalination, and film condensing device 303 concentrates, and finally obtains concentrate and is back to centrifuge washing leaching cake, or be back to crystallizer crystallization again.In addition, the strainer of filter 301 also receives the top stream clear liquid of concentrator, recycles this waste liquid by foregoing schemes; Strainer filters the filter residue (or dope) obtained, and is also back to crystallizer and uses as crystal seed.
Embodiment 1
Be described in detail referring to Fig. 8-11 pairs of the preferred embodiments of the present invention.The organic synthesis feed liquid of this embodiment iminodiacetonitrile obtains according to the production method of patent CN1331844C; The following sulfuric acid added, for the neutralization of ammonia in reaction system.The operation of unreceipted actual conditions in embodiment, conveniently operating condition is carried out.
By the material (material code name: FED1, wherein iminodiacetonitrile content is 300 g/L, temperature 65 DEG C, pH=7.0) of iminodiacetonitrile reactor extraction with 10.5 m
3the speed of/h is sent in dosage bunker 5 continuously, and the material simultaneously sent into continuously also comprises: product centrifugal filter cake washing lotion and secondary thickener underflow mixed liquor (material code name: FED 2; Wherein iminodiacetonitrile content is 50 g/L, temperature 12 DEG C, feed rate: 2 m
3/ h), the saturating washing lotion of nanofiltration (material code name: FED 3; Wherein iminodiacetonitrile content is 20 g/L, temperature 35 DEG C, feed rate: 3 m
3/ h), (temperature 25 DEG C, flow is about 0.22m to 93% sulfuric acid
3/ h).All materials mix in dosage bunker 5, and extraction is in film decolouring integrated system continuously, and in extraction material (code name FED 4), iminodiacetonitrile content is 140 g/L, and temperature 35 DEG C, extraction speed is about 15 m
3/ h.FED4 is successively by the ultrafiltration in film decolouring integrated system and nanofiltration process.(material code name FED5, iminodiacetonitrile content is 152 g/L to nanofiltration permeate, temperature 36 DEG C, and rate of feed is 9 m
3/ h) enter storage tank and (material code name FED6, iminodiacetonitrile content is 180 g/L, temperature 42 DEG C, flow 2.6 m at this and film concentrate
3/ h) mixing after, be pumped in crystal system and carry out crystallization; (material code name FED7, iminodiacetonitrile content is 2 g/L to nanofiltration trapped fluid, temperature 18 DEG C, flow 2.6 m
3/ h) enter temporary storage tank, and deliver to evaporimeter 7 and concentrate, incinerator 8 finally sent into by concentrate, with burning disposal after natural gas mixed aerosol; The saturating washing lotion of nanofiltration (material code name: FED 3; Wherein iminodiacetonitrile content is 20 g/L, temperature 35 DEG C) after collecting, return dosage bunker 5.This continuous crystallizing system is made up of MSMPR pattern crystallizer series connection DTB crystallizer, crystallized stock carries out crystallization by MSMPR pattern crystallizer and DTB crystallizer successively, temperature of charge in control DTB crystallizer is stable at 9 DEG C ~ 12 DEG C, pH value controls between 2.0 ~ 4.0, by regulating crystallizer feed rate, crystallized stock mean residence time is in a crystallizer made to be 1 to 3 hour.
Send in one-level concentrator by the magma of crystal system extraction, thickener underflow is the product magma of solid content 50% (V/V%), average crystal grain diameter is 0.3 more than mm, send into suspended centrifuge and carry out solid-liquid separation, obtain the solid product filter cake of moisture < 1% (w/w%), be packaged to be finished product by centrifuge automatic discharging, vibrations tape transport and automatic packaging machine.Centrifuge mother liquor (material code name: FED8; Wherein iminodiacetonitrile content is 60 g/L, temperature 12 DEG C) after collecting, be pumped to secondary concentrator.Top stream (material code name: FED 9 in one-level concentrator; Wherein iminodiacetonitrile content is 75 g/L, temperature 10 DEG C, flow: 10 m
3/ h) enter secondary concentrator with gravity current form.The underflow of secondary concentrator enters feeder 6, and mixes with product centrifugal filter cake washing lotion at this, and mixed liquor (FED2) returns dosage bunker 5, mixes with FED1 and FED3.Secondary concentrator top stream (material code name: FED 10; Wherein iminodiacetonitrile content is 65 g/L, temperature 12 DEG C, flow: 10 m
3/ h) filtered by leaf filter, clear liquid (material code name: the FED 11 obtained; Wherein iminodiacetonitrile content is 65 g/L, and ammonium sulphate content is: 20 g/L, temperature 12 DEG C, flow: 10 m
3/ h) enter electrodialysis desalination integrated system.
FED11 obtains two strands of materials after treatment: one is haline water (material code name: FED12, ammonium sulphate content 80 g/L), and send into evaporating, concentrating and crystallizing device, crystallization obtains solid ammonium sulfate product; Another strand of material is that (FED 13, iminodiacetonitrile content is 60 g/L to desalinization liquor, ammonium sulphate content 0.15 g/L, flow 10 m
3/ h), send into reverse osmosis membrane (RO film) concentration systems, (material code name FED6, iminodiacetonitrile content is 180 g/L, temperature 42 DEG C, flow 2.6 m to obtain material concentrate after treatment
3/ h) and fresh water (FED 15, flow 7.5 m
3/ h).Crystal system is entered after FED6 and FED5 mixing.
Compared with traditional handicraft, this technique has some main advantage following:
(1) large-scale industrial production, product yield, quality all have remarkable lifting, and in reactant liquor, product extraction efficiency is promoted to more than 95% by 80%, and the main content of product rises to 97% by average 95%, and outward appearance becomes near-white from brown.
(2) wastewater flow rate obviously declines, and product wastewater flow rate per ton is about 0.15 m
3, be only 1/10 of former technique, and waste water be high concentration without salting liquid, be easy to burning disposal.
(3) compared with former technique, the ammonium sulfate entering waste water is isolated, achieves recycling, reduce wastewater treatment difficulty simultaneously.
(4) traditional handicraft adopts repeatedly the mode of evaporation and concentration to take out, and consumes a large amount of steam; After adopting film concentration technique, concentrated expense greatly reduces.
(5) production overall process becomes continuous operation from intermittently operated, is easy to realize whole-course automation and controls, greatly reduce artificial use.
(6) traditional production technology due to product crystal grain little, Size Distribution is wide, cause product centrifugal filter cake water content on average more than 6.0%, this technique is due to lifting (the average crystal grain diameter increase of product crystalline quality, crystal size distribution scope is narrower), for iminodiacetonitrile, product filter cake can be made to be less than the moisture of 0.5% (w/w%) by means of only centrifugation, greatly be better than the quality index of Grade A moisture≤3.0% (w/w%) in GB/T23958-2009 " industrial iminodiacetonitrile ", thus centrifugal follow-up product drying operation in omission traditional handicraft, enormously simplify production procedure, reduce artificial consumption.
Embodiment 2
Be described in detail referring to Fig. 8-11 pairs of the preferred embodiments of the present invention.The organic synthesis feed liquid of this embodiment iminodiacetonitrile obtains according to the production method of patent CN1331844C; The following sulfuric acid added, for the neutralization of ammonia in reaction system.The operation of unreceipted actual conditions in embodiment, conveniently operating condition is carried out.
By the material (material code name: FED1, wherein iminodiacetonitrile content is 300 g/L, temperature 65 DEG C, pH=7.0) of iminodiacetonitrile reaction system extraction with 10.5 m
3the speed of/h is sent to dosage bunker 5 continuously.The material simultaneously continuously sent into also comprises: product centrifugal filter cake washing lotion and secondary thickener underflow through mixing, filter after clear liquid (material code name: the FED 2 that obtains; Wherein iminodiacetonitrile content is 50 g/L, temperature 12 DEG C, feed rate: 7.25 m
3/ h), mixed liquor (material code name: the FED 3 of UF membrane ultrafiltration and the saturating washing lotion of nanofiltration system; Wherein iminodiacetonitrile content is 30 g/L, temperature 35 DEG C, feed rate: 8.75m
3/ h), (temperature 25 DEG C, flow is about 0.185 m to 93% sulfuric acid
3/ h).Above-mentioned four kinds of materials enter preparation liquid storage tank after being mixed by one group of static mixer, and extraction is in film decolouring integrated system continuously, in extraction material (code name FED 4), iminodiacetonitrile content is for being 140 g/L, temperature 35 DEG C, extraction speed is about 26.5 m
3/ h.FED4 is successively by the ultra-filtration process in Integrated Films piece-rate system and nanofiltration process process.(material code name FED5, iminodiacetonitrile content is 138 g/L to nanofiltration permeate, temperature 36 DEG C, and rate of feed is 26.5 m
3/ h) enter storage tank; Meanwhile, by the mixed liquor of product centrifugal filter cake washing lotion and secondary thickener underflow, (material code name FED6, iminodiacetonitrile content is 350 g/L, temperature 20 DEG C, flow 2.2 m
3/ h) send into same storage tank, be pumped in crystal system after mixing and carry out crystallization.
The nanofiltration system of this example is made up of two kinds of films that pore size is different, the NF membrane composition one-level nanofiltration system that aperture is larger, the film composition secondary nanofiltration system that aperture is less.Solution after hyperfiltration treatment is successively by two-stage nanofiltration system.(iminodiacetonitrile content is 30 g/L to one-level nanofiltration trapped fluid, temperature 35 DEG C, flow 2 m
3/ h) enter temporary storage tank, and deliver to evaporimeter 7 and concentrate, incinerator 8 finally sent into by concentrate, with burning disposal after natural gas mixed aerosol; (wherein iminodiacetonitrile content is 40 g/L to secondary nanofiltration trapped fluid, ammonium sulphate content 70 g/L, temperature 35 DEG C, flow 4 m
3/ h) deliver to electrodialysis system and remove ammonium sulfate (in solution, ammonium sulphate content is 5 g/L after electrodialysis process) after collecting, then mix with one-level nanofiltration permeate, jointly enter secondary nanofiltration system.
Crystal system and later technical process identical with example 1.Finally, send in one-level concentrator by the magma of crystal system extraction, thickener underflow is the product magma of solid content 50% (V/V%), average crystal grain diameter is more than 0.3mm, send into suspended centrifuge and carry out solid-liquid separation, obtain the solid product filter cake of moisture < 1% (w/w%), be packaged to be finished product by centrifuge automatic discharging, vibrations tape transport and automatic packaging machine.In reactant liquor, product extraction efficiency is 96%, and the main content of product is 99%, and outward appearance is near-white.Product wastewater flow rate per ton is about 0.06m
3, be only 1/10 of former technique.
It should be noted that: the structure, ratio, size etc. of this description institute accompanying drawing; and the allocation and utilization of common apparatus; content all only in order to coordinate description to disclose; understand for person skilled in the art scholar and read; and be not used to the scope limiting the utility model enforcement; the adjustment of the modification of any structure, the change of proportionate relationship or size; and the increase and decrease of common apparatus and replacement; not affecting under the function that the utility model can produce and the object reached, all should drop in the protection domain of the technology contents that the utility model discloses.
The extraction index of above-described embodiment, system parameter setting and the amount adding sulfuric acid should not be defined as above-mentioned value, can need adjust according to concrete technology.The utility model is not limited to the production of iminodiacetonitrile, and other feed liquid system having similar composition also can adopt apparatus system of the present utility model and method to carry out separation and purification and liquid waste processing.Above embodiment is only in order to illustrate the technical solution of the utility model and unrestricted, although be described in detail the utility model with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify to the technical solution of the utility model or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present utility model.
Claims (12)
1. the separation and purification system of an organic synthesis feed liquid, comprise the crystal system (1) and solid-liquid separation system (2) that set gradually from front to back, it is characterized in that: described crystal system (1) is the continuous crystallizing system of at least two-stage crystallizer composition, is connected in series between described crystallizer.
2. the separation and purification system of organic synthesis feed liquid according to claim 1, it is characterized in that: described crystal system (1) is discharged crystallizer series connection guide shell crystallizer by mix suspending-product mix and formed, or discharge crystallizer by guide shell crystallizer series hybrid suspension-product mix to form, or discharge crystallizer by two or more mix suspending-product mix to be composed in series, or be composed in series by two or more guide shell crystallizer.
3. the separation and purification system of organic synthesis feed liquid according to claim 1, it is characterized in that: also comprise the liquid processing system (3) processed the liquid of solid-liquid separation system (2) extraction, this liquid processing system (3) comprises the desalter (302) and film condensing device (303) that set gradually from front to back; The filtrate (liquid of described solid-liquid separation system (2) is connected with the import of desalter (302), and the desalinization liquor outlet of described desalter (302) is connected with the import of film condensing device (303).
4. the separation and purification system of organic synthesis feed liquid according to claim 3, is characterized in that: described desalter (302) is electrodialysis plant or diffusion dialysis device.
5. the separation and purification system of organic synthesis feed liquid according to claim 3, is characterized in that: described solid-liquid separation system (2) comprises the concentrator and centrifuge that set gradually for more than a pair.
6. the separation and purification system of organic synthesis feed liquid according to claim 5, is characterized in that: described solid-liquid separation system (2) comprises the one-level concentrator, suspended centrifuge, secondary concentrator and the leaf filter that set gradually; The charging aperture of described one-level concentrator is connected with the discharging opening of crystal system (1), the thick material outlet of underflow of one-level concentrator is connected with the charging aperture of suspended centrifuge, and the top stream purified liquor outlet of one-level concentrator is connected with the charging aperture of secondary concentrator with the filtrate (liquid of suspended centrifuge; The thick material outlet of underflow of described secondary concentrator is connected with the charging aperture of crystal system (1), and the top stream purified liquor outlet of secondary concentrator is connected with the charging aperture of leaf filter; The filtrate (liquid of described leaf filter is connected with the charging aperture of desalter (302).
7. the separation and purification system of organic synthesis feed liquid according to claim 5, is characterized in that: the concentrated solution outlet of described film condensing device (303) is connected with the charging aperture of centrifuge and/or crystal system (1) crystallizer.
8. the separation and purification system of organic synthesis feed liquid according to claim 3, it is characterized in that: described crystal system (1) is front is provided with decolouring system (4), the destainer outlet of described decolouring system (4) is connected with the charging aperture of crystal system (1); Or, decolouring system (4) is provided with between described solid-liquid separation system (2) and desalter (302), now, the filtrate (liquid of described solid-liquid separation system (2) is connected with the import of decolouring system (4), and the destainer outlet of decolouring system (4) is connected with the import of desalter (302) again.
9. the separation and purification system of organic synthesis feed liquid according to claim 8, is characterized in that: described decolouring system (4) is made up of the ultrafiltration apparatus of connecting and nanofiltration device.
10. the separation and purification system of organic synthesis feed liquid according to claim 8, it is characterized in that: described desalter (302) is front is also provided with filter (301) or filtrate collecting tank (6), the filtrate (liquid of described solid-liquid separation system (2) is connected with the import of filter (301) or filtrate collecting tank (6) respectively, and the purified liquor outlet of described filter (301) or filtrate collecting tank (6) is connected with the import of desalter (302) again; When being provided with decolouring system (4) after solid-liquid separation system (2), the pretreatment part that described filter (301) is decolouring system (4), the filtrate (liquid of described solid-liquid separation system (2) is connected with the import of filter (301), and the purified liquor outlet of filter (301) is connected with the import of decolouring system (4) again.
The separation and purification system of 11. organic synthesis feed liquids according to claim 10, is characterized in that: the precipitation outlet of described filter (301) or filtrate collecting tank (6) is connected with the charging aperture of crystal system (1).
The separation and purification system of the organic synthesis feed liquid described in 12. any one of claim 3 to 11, it is characterized in that: described crystal system (1) is replaced by single crystallizer, or the crystal system that described crystal system (1) is composed in parallel by two or more crystallizer is replaced.
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| CN104744326B (en) | 2015-02-12 | 2016-08-10 | 山东新和成氨基酸有限公司 | Method for continuously preparing high-bulk-density methionine crystals |
| CN104707549B (en) * | 2015-03-19 | 2016-09-14 | 张汉文 | A kind of device and method reclaiming chromatographic grade organic reagent from organic reagent waste liquid |
| CN104844487A (en) * | 2015-04-05 | 2015-08-19 | 杭州蓝然环境技术有限公司 | Method for decoloring methionine crystallization mother liquor by adopting membrane integration technology |
| CN105566168A (en) * | 2015-12-28 | 2016-05-11 | 江苏远洋药业股份有限公司 | Creatine mother liquid separation purification processing system |
| CN105797876B (en) * | 2016-04-20 | 2018-06-29 | 贵州中伟正源新材料有限公司 | A kind of mother liquor material recycling device |
| CN108794364A (en) * | 2017-05-02 | 2018-11-13 | 宁夏紫光天化蛋氨酸有限责任公司 | A kind of isolation and purification method of methionine |
| CN108671578A (en) * | 2018-05-10 | 2018-10-19 | 江苏鼎烨药业有限公司 | One kind having impurity-eliminating effect and 2,4 dichloro phenol concentration and crystallization device easy to operation |
| CN108623651A (en) * | 2018-06-19 | 2018-10-09 | 南京肽业生物科技有限公司 | Efficient Peptide systhesis device |
| CN110937730A (en) * | 2019-05-08 | 2020-03-31 | 安阳师范学院 | Method for recovering organic nutrients and water in organic synthetic industrial waste |
| CN110812877B (en) * | 2019-10-12 | 2021-03-23 | 西安交通大学 | Glyphosate mother liquor treatment method and device |
| CN113044863B (en) * | 2021-04-25 | 2022-06-21 | 百色学院 | Method for improving decomposition rate of seed precipitation in alumina production |
| CN114314994A (en) * | 2022-02-17 | 2022-04-12 | 上海师范大学 | Device system and method for treating vitamin B6 production wastewater through membrane separation |
| CN114669076B (en) * | 2022-03-30 | 2023-03-28 | 上海东庚化工技术有限公司 | Micro-melt crystallization and falling film crystallization combined material purification system and method |
| CN115159756B (en) * | 2022-06-30 | 2023-09-01 | 江苏峻尚新材料科技有限公司 | Filtering assisting device and method for improving performance of ammonia desulfurization sewage slurry |
| CN116282689B (en) * | 2023-03-01 | 2023-10-13 | 广东工业大学 | Method and device for desalting high-salt high-concentration organic wastewater by coupling three membrane separation technologies |
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| JP2001321602A (en) * | 2000-05-15 | 2001-11-20 | Kurita Water Ind Ltd | Method and device for treating phosphorus-containing organic waste liquid |
| CN101139382A (en) * | 2007-09-30 | 2008-03-12 | 江南大学 | Method for separating and purifying glutathione in fermentation liquor by five-region simulated moving bed chromatography |
| CN101456822B (en) * | 2008-11-28 | 2012-07-25 | 山东恩贝生物工程有限公司 | Novel process for extracting threonine |
| VN29235A1 (en) * | 2009-06-04 | 2012-03-26 | ||
| CN101863783B (en) * | 2010-06-22 | 2013-05-01 | 华东理工大学 | Method for separating and purifying gamma-aminobutyric acid (GABA) from glutamine decarboxylase enzymolysis liquid |
| CN101982456A (en) * | 2010-09-25 | 2011-03-02 | 刘长飞 | Production method of environmental-friendly chloroacetic acid-process glycine |
| CN102924321B (en) * | 2012-11-30 | 2015-12-09 | 通辽梅花生物科技有限公司 | A kind of method extracting glutamine from fermented liquid |
| CN104058537B (en) * | 2014-04-30 | 2015-08-05 | 浙江工业大学 | A kind of method processing Cephalexin Monohydrate Micro/Compacted enzymatic clarification mother liquor waste water |
| CN104176844A (en) * | 2014-05-14 | 2014-12-03 | 重庆紫光化工股份有限公司 | Recycling system and recycling method for waste liquor produced in separation and purification of organically synthesized feed liquid |
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